CN108940315B - Bismuth vanadate powder for sterilizing nano array and preparation and application thereof - Google Patents
Bismuth vanadate powder for sterilizing nano array and preparation and application thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 52
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 35
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 35
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 230000001954 sterilising effect Effects 0.000 title abstract description 14
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- 238000001354 calcination Methods 0.000 claims abstract description 11
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
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- 239000002244 precipitate Substances 0.000 claims description 21
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 10
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 10
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- 238000000967 suction filtration Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
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- 230000000694 effects Effects 0.000 description 8
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- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 8
- 229940043267 rhodamine b Drugs 0.000 description 8
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
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- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- 102100030310 5,6-dihydroxyindole-2-carboxylic acid oxidase Human genes 0.000 description 5
- 101000773083 Homo sapiens 5,6-dihydroxyindole-2-carboxylic acid oxidase Proteins 0.000 description 5
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- SFOQXWSZZPWNCL-UHFFFAOYSA-K bismuth;phosphate Chemical compound [Bi+3].[O-]P([O-])([O-])=O SFOQXWSZZPWNCL-UHFFFAOYSA-K 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
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- NRGIRRZWCDKDMV-UHFFFAOYSA-H cadmium(2+);diphosphate Chemical compound [Cd+2].[Cd+2].[Cd+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O NRGIRRZWCDKDMV-UHFFFAOYSA-H 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
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- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 2
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- 239000004065 semiconductor Substances 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
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- 239000007832 Na2SO4 Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
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- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to the field of photocatalytic functional materials, and particularly relates to a bismuth vanadate powder for a bactericidal nano-array, and preparation and application thereof. The general formula of the bismuth vanadate powder of the bactericidal nano array is as follows: (BiVO)4)x/(CdS)y,0<x:y<1. The powder has high photocatalytic efficiency, a sterilization function, a simple and easy preparation process, low calcination temperature, mild and easy control conditions, excellent performance of the prepared sample, low cost and suitability for large-scale production.
Description
Technical Field
The invention belongs to the field of photocatalytic functional materials, and particularly relates to a bismuth vanadate powder for a bactericidal nano array and a preparation and application technology thereof.
Background
Water is the most important substance for human life, production and life, and the water quality and water purification problems directly affect the daily production and life of national economy and the nation. Untreated dye wastewater is directly discharged into rivers, lakes and seas, and can seriously pollute surface water resources and underground water resources, so that not only are available water resources less and less, but also a great amount of deformity and death of aquatic organisms are caused. Therefore, high and new technologies capable of effectively degrading dyes in wastewater should be rapidly researched.
Bismuth vanadate (BiVO)4) Has attracted great interest due to its unique properties, such as excellent visible light response, low band gap, diverse morphology and relatively high photocatalytic water splitting activity, and can be used for degrading organic compounds, inactivating bacteria, etc. But its poor separation ability of electron-hole pairs and low utilization of visible light results in its poor photocatalytic ability. Therefore, people adopt control of the form, doping of metal and nonmetal elements, construction of semiconductor heterojunction and the like to improve the photocatalytic performance of the semiconductor heterojunction. For example, Weeket al [1 ]]([1] BiVO4 nanowires decorated with CdS nanoparticles as Z-scheme photocatalyst with enhanced H2 generation)V2O5And Na2SO4Hydrothermally produced Na2V6O16·3H2O nanowire and Bi (NO)3)3·5H2O mixing and solvothermal preparation of BiVO4A nanowire. With Na2S·9H2O and Cd (Ac)2·2H2And preparing CdS nano-particles by a O hydrothermal method. Finally BiVO4The nano wire and CdS nano particle are dispersed in glycol by ultrasonic, and 1D CdS/BiVO is prepared by glycol solvothermal method4A nanowire. In middle aged people [2]([2] High Efficient Photodegradation and Photocatalytic Hydrogen Production of CdS/BiVO4 Heterostructure through Z-scheme Process)Bi(NO3)3·5H2O and NH4VO3Preparing BiVO4 nanosheets by a solvothermal method under the condition of pH =6.5, and then mixing the nanosheets with Cd (CH)3COO)2Mixing with thiourea, and preparing CdS/BiVO4 heterojunction under heating condition.
In the preparation process, the former mainly works on the appearance, the performance and the preparation method, and the control of interface electron flow direction and photoacoustic electron separation and recombination is not fundamentally solved. Therefore, the development of a controllable nano-array bismuth vanadate powder and the preparation and application thereof become problems to be solved urgently at present.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method and application of bismuth vanadate powder for a bactericidal nano array. The powder has high photocatalytic efficiency, a sterilization function and a simple preparation method, and is a novel photocatalytic and sterilization nano material.
In order to achieve the above object, the invention provides a bismuth vanadate powder for bactericidal nanoarray, which has a general formula: (BiVO)4)x/(CdS)y, 0<x:y<1。
Preferably, the chemical formula of the powder is as follows: (BiVO)4)x/(CdS)y,x:y=2:3。
A preparation method of bismuth vanadate powder for a bactericidal nano array comprises the following steps:
step 3, dissolving soluble salt of Cd in deionized water, dripping the solution into the solution B under the ultrasonic condition, keeping ultrasonic for 0.5-1 hour, and then dripping Na2Keeping the solution of S in an ultrasonic state for 0.5-1 hour, adding a certain amount of dispersant, and performing suction filtration to obtain a precipitate C;
step 4, putting the precipitate C into an oven for drying treatment;
and 5, putting the dried precipitate into a muffle furnace for calcining, and preserving heat to obtain the nano-array bismuth vanadate powder.
In the step (1), the soluble salt of Bi is one of chloride, acetate, nitrate, phosphate and the like. The dosage of the glycol solution is 10 to 20 times of the molar dosage of the Bi soluble salt.
In the step (2), the stirring speed is 500r/min-800 r/min.
NH in the step (2)4VO3The molar ratio of the amount of the Bi salt to the amount of the Bi salt is 1: 1; the dosage of the deionized water is 10-3 of the molar dosage of the Bi soluble salt0 times.
The dosage of the deionized water in the step (3) is 10-20 times of the molar dosage of the Cd soluble salt. Cd [ Cd ]2+:S2-1: 1; the dispersant is dimethylglyoxime, and the dosage of the dispersant is 0.2 to 0.5 time of the molar dosage of the Cd soluble salt.
In the step (4), the drying temperature is 70-90 ℃, and the drying time is 1-2 h.
The calcination temperature in the step (5) is 400-500 ℃, and the heat preservation is carried out for 1-2 hours.
The bactericidal nano array bismuth vanadate powder is applied to preparing an organic matter degradation agent or a bactericide.
Compared with the prior art, the invention has the beneficial effects.
The nano-array bismuth vanadate powder prepared by the invention has unique morphology, effectively solves the problems of interface electron flow direction and photoacoustic electron separation and compounding, has excellent visible light response, and has high powder purity and good catalytic performance.
The invention focuses on crystal face control and design, so that different crystal faces are exposed under different conditions, and the directional growth of the crystal faces is controlled, so that the crystal faces have higher reaction activity. And practice and regulation are carried out on the sterilization performance, so that the sterilization composite material has multiple effects and meets the requirement of environmental protection.
According to the invention, through adding a dispersant CTAB, simultaneously adopting a Soxhlet extractor for extraction and preparation, reacting at a high temperature (80-100 ℃), adding CTAB, and controlling reflux time, the adsorption degree of CTAB on the surface of BiVO4 is changed, the growth of (010) and (101) surfaces is inhibited by the change, so that the (010) and (101) surfaces are reserved, the appearance of a sample is accurately controlled, and the directional growth of the CTAB to different crystal surfaces under different conditions is controlled, so that the CTAB has higher reactivity.
The photocatalyst nano-array powder has a relatively obvious catalytic effect on rhodamine B. The invention also provides a preparation method of the nano-array bismuth vanadate powder, the preparation process is simple and easy to operate, the calcination temperature is low, the conditions are mild and easy to control, and the prepared sample has excellent performance and low cost and is suitable for large-scale production. And can be used for degrading organic compounds, inactivating bacteria, etc.
Drawings
FIG. 1 is an XRD pattern of a sample prepared in example 1;
FIG. 2 is an SEM image of a sample prepared in example 2;
FIG. 3 is an SEM image of a sample prepared in example 3;
FIG. 4 is a diagram of the photocatalytic degradation of rhodamine B by samples prepared in example 4;
FIG. 5 is a graph of data from the bacterial experiment of example 5;
FIG. 6 is an SEM image of a sample prepared in comparative example 1;
fig. 7 is an SEM image of a sample prepared in comparative example 2.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
A bismuth vanadate powder for sterilizing nano arrays has a general formula as follows: (BiVO)4)x/(CdS)y, 0<x:y<1。
The preparation method of the bismuth vanadate powder for the bactericidal nanoarray comprises the following steps:
step 1: weighing 0.6mmol of bismuth nitrate, dissolving the bismuth nitrate in a certain amount of glycol solution (the volume of the glycol is 20 times of the molar weight of the bismuth nitrate), adding 0.1g of CATB, and stirring to obtain a solution A;
step 2: weighing 0.6mmol NH4VO3Dissolving in deionized water (the volume of the deionized water is 15 times of the molar weight of the bismuth nitrate), stirring at 500r/min for 0.5h, and placing the dissolved liquid into an extraction tube of a Soxhlet extractor. Slowly pouring the solution A into a flask at the upper end of a Soxhlet extractor, refluxing for 0.5 hour at 100 ℃, and cooling to obtain a solution B.
And step 3: weighing 0.9mmol of cadmium nitrate, dissolving the cadmium nitrate in deionized water (the volume usage of the deionized water is 10 times of the molar weight of the cadmium nitrate), dripping the solution into the solution B, keeping ultrasonic for 30 minutes, and then dripping Na2Keeping the solution S under ultrasonic treatment for 1 hour, adding 0.18mmol of dimethylglyoxime dispersant, carrying out suction filtration treatment,obtaining a precipitate C;
step 4, putting the precipitate C into a drying oven, and drying for 2 hours at 70 ℃; and (3) calcining the dried precipitate in a muffle furnace at 450 ℃, and preserving heat for 1h to obtain the nano-array bismuth vanadate powder.
The XRD pattern of the obtained powder is shown in figure 1, and the prepared powder is relatively pure.
Example 2
A bismuth vanadate powder for sterilizing nano arrays has a general formula as follows: (BiVO)4)x/(CdS)y, 0<x:y<1。
The preparation method of the bismuth vanadate powder for the bactericidal nanoarray comprises the following steps:
step 1: weighing 0.5mmol of bismuth acetate, dissolving the bismuth acetate in a certain amount of ethylene glycol solution (the volume of the ethylene glycol is 15 times of the molar amount of the bismuth acetate), adding 0.1g of CATB, and stirring to obtain a solution A;
step 2: weighing 0.5mmol NH4VO3Dissolving in deionized water (the volume of the deionized water is 10 times of the molar weight of the bismuth acetate), stirring at 600r/min for 0.5h, and placing the dissolved liquid into an extraction tube of a Soxhlet extractor. Slowly pouring the solution A into a flask at the upper end of a Soxhlet extractor, refluxing for 1 hour at 80 ℃, and cooling to obtain a solution B.
And step 3: weighing 1mmol of cadmium acetate, dissolving in deionized water (the volume usage of the deionized water is 10 times of the molar weight of the cadmium acetate), dripping the solution into the solution B, maintaining ultrasonic for 30 minutes, and dripping 1mmol of Na2Keeping the solution S in an ultrasonic state for 30 minutes, adding 0.5mmol of dimethylglyoxime dispersant, and performing suction filtration to obtain a precipitate C;
step 4, putting the precipitate C into an oven, and drying for 1h at 90 ℃; and putting the dried precipitate into a muffle furnace, calcining at 500 ℃, and preserving heat for 2h to obtain the nano-array bismuth vanadate powder.
The scanning electron microscope of the obtained powder is shown in FIG. 2.
Example 3
A bismuth vanadate powder for sterilizing nano arrays has a general formula as follows: (BiVO)4)x/(CdS)y, 0<x:y<1。
The preparation method of the bismuth vanadate powder for the bactericidal nanoarray comprises the following steps:
step 1: weighing 1.2mmol of bismuth phosphate, dissolving the bismuth phosphate in a certain amount of ethylene glycol solution (the volume of the ethylene glycol is 10 times of the molar weight of the bismuth phosphate), adding 0.1g of CATB, and stirring to obtain a solution A;
step 2: weighing 1.2mmol NH4VO3Dissolving in deionized water (the volume of the deionized water is 20 times of the molar weight of the bismuth phosphate), stirring at 800r/min for 0.5h, and placing the dissolved liquid into an extraction tube of a Soxhlet extractor. Slowly pouring the solution A into a flask at the upper end of a Soxhlet extractor, refluxing for 1 hour at 90 ℃, and cooling to obtain a solution B.
And step 3: weighing 1.8mmol of cadmium phosphate, dissolving the cadmium phosphate in deionized water (the volume usage of the deionized water is 10 times of the molar weight of the cadmium phosphate), dripping the solution into the solution B, keeping ultrasonic for 60 minutes, and then dripping Na2Keeping the solution S in an ultrasonic state for 1 hour, adding 0.54mmol of dimethylglyoxime dispersant, and performing suction filtration to obtain a precipitate C;
step 4, putting the precipitate C into an oven, and drying for 2 hours at the temperature of 80 ℃; and putting the dried precipitate into a muffle furnace, calcining at 400 ℃, and preserving heat for 1h to obtain the nano-array bismuth vanadate powder.
The scanning electron microscope of the obtained powder is shown in FIG. 3. As can be seen from fig. 3, the bismuth vanadate powder having the nano array can be prepared. As shown in fig. 3, in the present embodiment, CTAB is added, and a reflux reaction is performed at a high temperature of 90 ℃, so that the degree of CTAB adsorption on the surface of BiVO4 changes, and the change inhibits the growth of the (010) plane, so that the (010) plane is retained, the morphology of the sample is accurately controlled, and the sample is controlled to directionally grow to different crystal planes under different conditions, so that the sample has higher reactivity.
Compared with the prior art, the directionally-grown nano powder prepared by the invention has larger specific surface area and more reactive active sites, thereby improving the capacity of degrading RhB, and the bismuth vanadate powder consisting of the homodromous growth array is not reported.
Example 4
A bismuth vanadate powder for sterilizing nano arrays has a general formula as follows: (BiVO)4)x/(CdS)y, 0<x:y<1。
The preparation method of the bismuth vanadate powder for the bactericidal nanoarray comprises the following steps:
step 1: weighing 1mmol of bismuth nitrate, dissolving the bismuth nitrate in a certain amount of ethylene glycol solution (the volume of the ethylene glycol is 15 times of the molar weight of the bismuth nitrate), adding 0.1g of CATB, and stirring to obtain a solution A;
step 2: weighing 1mmol NH4VO3Dissolving in deionized water (the volume of the deionized water is 30 times of the molar weight of the bismuth nitrate), stirring at 700r/min for 1h, and putting the dissolved liquid into an extraction tube of a Soxhlet extractor. Slowly pouring the solution A into a flask at the upper end of a Soxhlet extractor, refluxing for 0.5 hour at 100 ℃, and cooling to obtain a solution B.
And step 3: weighing 5mmol of cadmium nitrate, dissolving the cadmium nitrate in deionized water (the volume usage of the deionized water is 10 times of the molar weight of the cadmium nitrate), dripping the solution into the solution B, keeping ultrasonic for 60 minutes, and then dripping Na2Keeping the solution S in an ultrasonic state for 1 hour, adding 1mmol of dimethylglyoxime dispersant, and performing suction filtration to obtain a precipitate C;
step 4, putting the precipitate C into an oven, and drying for 1.5h at 70 ℃; and (3) calcining the dried precipitate in a muffle furnace at 450 ℃, and preserving heat for 1.5h to obtain the nano-array bismuth vanadate powder.
Testing the effect of degrading rhodamine B by photocatalysis of a sample with the same concentration by adopting an ultraviolet-visible light photometer, and finally performing drawing analysis by using Origin software; preparing a rhodamine B solution: weighing 0.05g of rhodamine B powder, dissolving the rhodamine B powder in 100ml of deionized water, diluting 5ml of solution in 45ml of distilled water to prepare 50ml of diluent with the concentration of 50mg/L, and weighing 0.01g of powder samples with different doping proportions respectively in each catalytic experiment; and respectively observing the catalytic performance of the rhodamine B under the irradiation of a high-pressure mercury lamp of a multi-channel photocatalytic reactor after ultrasonic oscillation.
As shown in FIG. 4, it is clear that the powder has a relatively significant catalytic effect on rhodamine B. This increase in photocatalytic performance is mainly due to two aspects: 1. the built-in electric field at the interface promotes the separation of the photo-generated electron/hole pairs, and effectively reduces the recombination rate. 2. The surface activity of the photocatalyst is improved by the improvement of the appearance, the directional growth of the material, the flow direction of interface electrons and the separation and recombination of photoacoustic electrons.
Example 5
A bismuth vanadate powder for sterilizing nano arrays has a general formula as follows: (BiVO)4)x/(CdS)y, 0<x:y<1。
The preparation method of the bismuth vanadate powder for the bactericidal nanoarray comprises the following steps:
step 1: weighing 2mmol of bismuth acetate, dissolving the bismuth acetate in a certain amount of ethylene glycol solution (the volume of the ethylene glycol is 20 times of the molar amount of the bismuth acetate), adding 0.1g of CATB, and stirring to obtain a solution A;
step 2: weighing 2mmol NH4VO3Dissolving in deionized water (the volume of the deionized water is 20 times of the molar weight of the bismuth acetate), stirring at 700r/min for 0.5h, and placing the dissolved liquid into an extraction tube of a Soxhlet extractor. Slowly pouring the solution A into a flask at the upper end of a Soxhlet extractor, refluxing for 1 hour at 100 ℃, and cooling to obtain a solution B.
And step 3: weighing 3mmol of cadmium acetate, dissolving in deionized water (the volume usage of the deionized water is 10 times of the molar weight of the cadmium nitrate), dripping the solution into the solution B, maintaining ultrasonic for 30 minutes, and then dripping Na2Keeping the solution S in an ultrasonic state for 30 minutes, adding 1.5mmol of dimethylglyoxime dispersant, and performing suction filtration to obtain a precipitate C;
step 4, putting the precipitate C into an oven, and drying for 1h at 70 ℃; and putting the dried precipitate into a muffle furnace, calcining at 500 ℃, and preserving heat for 1.5h to obtain the nano-array bismuth vanadate powder.
The catalyst powder was subjected to a sterilization test. All glassware and water were disinfected prior to the antimicrobial test. 650ml of deionized solution, a small amount of bacteria stock solution is added and mixed evenly to ensure that the bacteria are evenly dispersed in 650ml of solution. 100ml of the bacterial stock was injected into each tube in the parallel screening machine. Several small tubes containing 9ml of deionized water were prepared for dilution. Two groups of parallel samples are taken for each sample to be measured, the conditions are completely consistent, and an averaging method is adopted during counting. FIG. 5 shows the effect of killing Escherichia coli at different times. The results show that the powder has obvious effect of killing escherichia coli, the better effect can be achieved within 30 minutes, and the escherichia coli can be completely killed within about 90 minutes.
Comparative example 1
Prepared into BiVO through a hydrothermal method4And nanowires are deposited, and CdS quantum dots are deposited by a simple deposition method to construct a Z-shaped heterostructure. 1mmol V2O5And 2mmolNa2SO4Dissolved in 40mL of deionized water. The mixture was then transferred to a 50mL autoclave and incubated at 180 ℃ for 24 h. The obtained Na2V6O16·3H2O nanowire and Bi (NO)3)3·5H2O is mixed in a molar ratio of 1: 6 dispersed in 40mL volume ratio of 4: 1 ethanol-water solution, then incubated at 120 ℃ for 24h in a 50mL autoclave to obtain BiVO4A nanowire.
CdS nanoparticles were synthesized by mixing 0.01mol of Na2S & 9H2O and 0.01mol of Cd (Ac) 2 & 2H2O in 40mL of water. The obtained CdS nano-particles are centrifuged, washed by deionized water and dried under the vacuum condition of 50 ℃.
By mixing CdS nano-particles and 1D BiVO in different weight ratios4The nanowires were ultrasonically dispersed in 40mL ethylene glycol and heated at 200 ℃ for 72h in a 50mL Teflon-lined autoclave to synthesize 1D CdS/BiVO4A nanowire. The scanning electron micrograph is shown in FIG. 6.
Comparative example 2
First using Bi (NO)3)3·5H2O and NH4VO3Preparing BiVO4 nanosheets by a solvothermal method under the condition of pH =6.5, and then mixing the nanosheets with Cd (CH)3COO)2And mixing the CdS/BiVO4 heterojunction with thiourea under a heating condition.
0.97gBi (NO)3)3·5H2O and0.5gC18H29NaO3s (SDBS) dissolved in 20mL HNO3(4mol L-1) To form a clear solution. Then dissolved in 20mL of NaOH solution (2mol L) under magnetic stirring-1) 0.234gNH in (1)4VO3Added dropwise to the above solution. After 0.5h, use NaOH solution (2mol L)-1) The pH of the mixed solution was adjusted to 6.5. The resulting material was transferred to a 100mL Teflon lined stainless steel autoclave and held at 160 ℃ for 1 hour. The product was collected by centrifugation, washed with distilled water and absolute ethanol, and then dried at 100 ℃ for 4 hours.
Adding 1mmol of Cd (CH)3COO)2Dissolved in 50mL of deionized water and obtained BiVO with different masses4The powders (25 mg, 50mg, 75mg and 100 mg) were dispersed in the above solution under sonication for 0.5 hour. Then 10mL of an aqueous solution of thiourea (0.1M) was poured and mixed with vigorous stirring. After 20 minutes, the mixture was heated at 90 ℃ for 2.5 h. Finally, the product was collected by centrifugation, washed with distilled water and absolute ethanol, and then dried at 70 ℃ overnight. The scanning electron micrograph is shown in FIG. 7.
The methods adopted in the 2 comparative examples are all prepared by a hydrothermal method, and the results show that the prepared CdS/BiVO4The appearance and the performance are substantially different from the appearance and the performance of the alloy. In comparative example 1, although the morphology is uniform and the single dimension is large, the composite interface with different morphologies is not completely represented, and the photo-etching of CdS is severe. In addition, the sintering agglomeration of the sheets was severe in comparative example 2. If the photocatalyst particles are too large, the catalytic area is small, and the number of active sites is small; the CdS particles are too fine, the built-in electric field is not favorable for charge separation, the anti-solubility is reduced, and the stability of the photocatalyst is poor. The hydrothermal method has low preparation yield, needs reaction at high temperature and high pressure, and has harsh conditions.
The patent adopts a simple normal-temperature two-step ultrasonic method to prepare the nano array with directional growth, the interface electron mobility is good, and the photoacoustic electrons are easier to separate. High-pressure heating and pH value regulation are not needed, the preparation method is simple, the Soxhlet extractor is adopted for extraction and preparation, the yield of the product is high, the purity of the sample is good, and the product has a sterilization effect on microorganisms.
Claims (9)
1. A preparation method of bismuth vanadate powder for a bactericidal nano array is characterized in that the general formula of the powder is as follows: (BiVO)4)x/(CdS)y,0<x:y<1, the preparation method of the bismuth vanadate powder for the bactericidal nanoarray comprises the following steps:
step 1, dissolving soluble salt of Bi in a certain amount of glycol solution, adding 0.1g CTAB, and stirring to obtain a solution A;
step 2, adding a certain amount of NH4VO3Dissolving in deionized water, magnetically stirring, placing into an extraction tube of a Soxhlet extractor, slowly pouring the solution A into a flask at the upper end of the Soxhlet extractor, refluxing at 80-100 deg.C for 0.5-1 hr, and cooling to obtain solution B;
step 3, dissolving soluble salt of Cd in deionized water, dripping the solution into the solution B under the ultrasonic condition, keeping ultrasonic for 0.5-1 hour, and then dripping Na2Keeping the solution of S in an ultrasonic state for 0.5-1 hour, adding a certain amount of dispersant, and performing suction filtration to obtain a precipitate C;
step 4, putting the precipitate C into an oven for drying treatment;
and 5, putting the dried precipitate into a muffle furnace for calcining, and preserving heat to obtain the nano-array bismuth vanadate powder.
2. The method of claim 1, wherein the powder has the formula: (BiVO)4)x/(CdS)y,x:y=2:3。
3. The preparation method of claim 1, wherein the soluble salt of Bi in step 1 is one of chloride, acetate, nitrate and phosphate, and the amount of the ethylene glycol solution is 10-20 times of the molar amount of the soluble salt of Bi.
4. The method of claim 1, wherein the step of preparing the composition comprisesIn said step 2, NH4VO3The molar ratio of the amount of the Bi salt to the amount of the Bi salt is 1: 1; the dosage of the deionized water is 10 to 30 times of the molar dosage of the Bi soluble salt.
5. The preparation method of claim 1, wherein the soluble salt of Cd in the step 3 is one of chloride, nitrate and phosphate; the dosage of the deionized water is 10-20 times of the molar dosage of the soluble salt of Cd, and Cd2+:S2-=1:1。
6. The method of claim 1, wherein the dispersant is dimethylglyoxime and the amount of the dispersant is 0.2 to 0.5 times the molar amount of the Cd soluble salt.
7. The preparation method according to claim 1, wherein the drying temperature in the step 4 is 70-90 ℃ and the drying time is 1-2 h; the calcination temperature in the step 5 is 400-500 ℃, and the heat preservation time is 1-2 hours.
8. The method of claim 1, wherein the stirring speed is from 500r/min to 800 r/min.
9. The application of the nano-array bismuth vanadate powder prepared by the preparation method of claim 1 in preparing organic degradation agents or bactericides.
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